CN101045799A - Preparation method of reclaimed rubber using microwave desulfurization method - Google Patents
Preparation method of reclaimed rubber using microwave desulfurization method Download PDFInfo
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- CN101045799A CN101045799A CNA2007100088440A CN200710008844A CN101045799A CN 101045799 A CN101045799 A CN 101045799A CN A2007100088440 A CNA2007100088440 A CN A2007100088440A CN 200710008844 A CN200710008844 A CN 200710008844A CN 101045799 A CN101045799 A CN 101045799A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
This invention relates to preparation method of a kind of regenerated rubber, adopts microwave devulcanization process. It adopts microwave desulfurization method and mechanical desulfurization method, carry out desulfuration to scrap tire and scrap rubber by rubber power or colloidal particle form. The products can 100 percent substitute new rubber, as raw material of shoemaking or rubber goods. The process includes: shatter scrap rubber to gain power, transit 5 to 200 times screening; use magnetism method for removeing iron leavings and impurity; Then put the rubber power to microwave devulcanizing pan, add rubber emollient; the mass ratio of rubber powder and emollient is 100: 0 to 15; microwave heating desulfuration, heating temperature is 140 to 300 deg; cooling to 150 deg after desulfuration completed, roll and milling for piece.
Description
Technical field
The present invention relates to a kind of preparation of reclaimed rubber, especially relate to a kind of method that adopts microwave desulfurization to prepare reclaimed rubber.
Background technology
Waste old is mainly derived from rubber items such as damaged tire, scrap rubber footwear and waste tape, next derives from scrap stock and the waste product that produces in the rubber production process, it belongs to the big class of one in the industrial solid wastes, but, caused the concern of countries in the world as the recycling of resource utilization macromolecular material.The growing amount of the annual junked tire of China is 2,200,000 tons, adds the scrap stock and the rubber waste product of shoemaking and other rubber item enterprises, and the waste rubber total amount reaches more than 3,000,000 tons, and increases with the speed in every year about 25%.The long-term air storage of these waste rubbers takies a large amount of soils, contaminate environment, easily initiation fire.On the other hand, the main raw material about 70% of producing tire and rubber item derives from the product of refining of petroleum, and the price and the oil price of rubber raw materials go up synchronously, have obviously reduced the productive profit of shoemaking and other rubber item enterprises.Waste rubber has the multiple approach that utilizes, but considers that from the angle of renewable resource and recycling economy it is the most reasonable to produce reclaimed rubber, and waste rubber almost 100% can utilize.The method that waste old is produced reclaimed rubber through desulfurization mainly contains chemistry and physical method two classes, China produces the method for reclaimed rubber at present based on the dynamic desulfurization of the High Temperature High Pressure in the chemical method, and this method not only energy consumption is big, and the production time is long, production efficiency is low, and has secondary pollution.
Microwave desulfurization is the novel method that adopted the rubber recycle in recent years in the world, and the U.S. has suitability for industrialized production.This method is a kind of on-mechanical, a step renovation process non-chemically, and it utilizes the C-S key and the S-S key of microwave energy cut-out sulfuration waste rubber, only needs the micelle with 6～8mm, and the time is short, and less energy consumption is pollution-free, and superior product quality can the new rubber of 100% replacement.Microwave desulfurization is one of best approach of producing high-quality and low-cost reclaimed rubber, has good industrial prospect.
Meijiang Jiaying Rubber-Plastic Plant, Meizhou City provides a kind of method of waste old desulfurization regeneration in the application for a patent for invention of publication number for CN1103350, especially utilize microwave and infrared heat reservoir, with suitable cooperation, the waste vulcanized rubber powder of interval re-treatment, the method for producing reclaimed rubber.Owing at interval microwave, infrared heat preservation zone are set, can regulate the microwave energy of each radiation zone, make dissimilar rubber powders, in different zones, obtain enough energy, reach the purpose of scission of link.Rubber powder adopts microwave radiation and infrared rays insulation processing at interval, and through stirring stirring, and heat, the rubber powder part of having avoided high-energy radiation of microwave to accumulate be overheated, be clamminess, smolder even charing, and the reclaimed rubber of production meets standard GB/T13460-92.
Hyundai Motor Corporation provides a kind of apparatus and method of handling surface of waste rubber powder with microwave continuous ground in the application for a patent for invention of publication number for CN1733443, it handles surface of waste rubber powder continuously by microwave device, thus the surface that makes it can be continuously and more effectively handle waste Crumb rubber.Therefore, reclaim elastomeric material and have surface of good roughness and processability, and the physics of described rubber item and chemical property all are improved.
Meijiang Jiaying Rubber-Plastic Plant, Meizhou City provides a kind of waste old desulfurizer in the utility model patent of publication number for CN2175680, form by body, feeding conveyor, outfeed belt conveyor, microwave heater and infrared tube, conveying belt places in the body, the conveying belt front end is a feeding conveyor, the other end is an outfeed belt conveyor, and infrared tube is above conveying belt.Owing to utilize microwave and infrared heat reservoir, the re-treatment waste rubber powder is produced reclaimed rubber, thereby is not had contaminated wastewater, and can directly penetrate rubber powder inside at interval, makes the rubber powder of the low property led can rapid and uniform heating, have simple in structure, the characteristics of being convenient to operate.
Summary of the invention
The present invention aims to provide a kind of reclaimed rubber preparation method who realizes the employing microwave desulfurization of rubber recycle suitability for industrialized production.Technical scheme of the present invention is to adopt microwave desulfurization and mechanical doctor treatment, damaged tire and waste rubber product are carried out desulfurization with the form of rubber powder or micelle after, 100% replaces new rubber, as the raw material of shoemaking or rubber item.
The present invention includes following steps:
1) the waste old material is pulverized waste rubber powder, cross 5～200 mesh sieves;
2) waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron;
3) waste rubber powder behind de-iron bits and the impurity is packed into microwave desulfurization jar, the adding Rubber Softener is pressed mass ratio, waste rubber powder: Rubber Softener=100: (0～15);
4) microwave heating desulfurization, 140～300 ℃ of Heating temperatures;
5) after desulfurization is finished, be cooled to below 150 ℃ roller refining, slice.
The waste old material package is drawn together rubber items such as damaged tire, scrap rubber footwear and waste tape, and scrap stock that produce in the rubber production process and waste product etc.The kind of waste old comprises natural rubber, styrene-butadiene rubber(SBR), cis-1,4-polybutadiene rubber, isoprene-isobutylene rubber, chloroprene rubber and paracril etc.The microwave frequency of the microwave that is adopted is 915～2450MHz, is preferably 945MHz, and microwave intensity is 0.1～1.0KWh/Kg, and the microwave desulfurization time is 5～40min, and microwave heating temperature is preferably 160～180 ℃.Rubber Softener is selected at least a in Stockholm tar, Yatall MA, turps, rosin, di-terpene, coal tar, the heavy oil etc. for use.
Microwave desulfurization equipment of the present invention can adopt general microwave desulfurization device, comprise microwave desulfurization jar, microwave generator, microwave transmission pipeline, whipping appts, microwave and temperature controlling system etc., for example adopt the 915MHz-20kW type microwave desulfurization device of prestige micro-wave energy company of Guangzhou section product etc.
Because the heat that desulfurization produced is bigger, very easily occurs the thermal dispersion effect during microwave desulfurization, i.e. the ability of medium absorption microwave is opened height with the temperature of medium and is increased.The particle diameter of micelle is big more, and the easy more internal temperature that causes is opened height and caused burning.Very easily cause spontaneous combustion because of oxidation.The method that solves has: leave standstill cooling back discharging after 1. desulfurization is finished under the condition of secluding air.2. behind the spray cooling, refining again, following sheet.Water spraying time length is with till reaching the temperature that stops oxidation.
Compare with existing reclaimed rubber preparation method, the present invention adopts the low frequency desulfurization because the utilization microwave desulfurization carries out the recycle of waste old, does not only heat, only need at room temperature carry out, and do not add infrared heat preservation zone, and needn't starvation, not spontaneous combustion of product, avoided the color and luster blackening, do not influence the requirement of reclaimed rubber, do not have obvious smell, help environmental protection color.After damaged tire and waste rubber product carried out desulfurization with the form of rubber powder or micelle, 100% replaced new rubber, as the raw material of shoemaking or rubber item, realizes the suitability for industrialized production of rubber recycle.Its technology is simple, and equipment cost is low, reclaims colloid amount height, and therefore the output height has very high economic benefit and environmental benefit, has a extensive future, and has a high potential.This shows that the useless sole scrap stock that utilize microwave desulfurization that waste old etc. especially white carbon black is filled carry out desulfurization, have solved the difficult problem that industrial other way is difficult to reclaim fast this type of waste rubber.
Embodiment
Embodiment 1: the shoes-used glue scrap stock belong to the white carbon black infill system, and its white carbon black content accounts for 40%～60%.The thermal dispersion effect of its microwave is not obvious, and desulfurization is even, but because the microwave heating effect of white carbon black is not obvious, desulfurization time is generally at 5～40min.Intend adopting step microwave desulfurization technology, temperature is controlled between 140～300 ℃, and temperature is low excessively, and the non-thermal effect of microwave is not enough to provide the fracture of vulcanization crosslinking network; And temperature is too high, surpasses the fracture activation energy of C-C key, and rubber backbone is destroyed serious, make C-S and S-S bond rupture, will (165～200 ℃) carry out desulfurization under suitable temperature.
Present embodiment adopts the footwear scrap stock, adds the tenderizer Stockholm tar, and desulfurization 20min gained reclaimed rubber is cooled to room temperature under refrigerating unit under the microwave radiation of 915MHz, and the experimental result that the reclaimed rubber that obtains cooperates with natural rubber is as shown in table 1.
Table 1
| NR consumption/phr | 100 | 90 | 70 | 50 | 20 | 0 |
| Desulfurization glue amount/phr | 0 | 10 | 30 | 50 | 80 | 100 |
| Minimum torque/Nm | 3.95 | 5.06 | 5.60 | 7.65 | 6.48 | 8.87 |
| Torque capacity/Nm | 7.66 | 8.75 | 8.42 | 9.99 | 8.24 | 9.99 |
| T S2/min | 1.38 | 1.32 | 1.30 | 1.33 | 1.62 | 1.92 |
| T 90/min | 2.18 | 2.63 | 4.41 | 5.75 | 7.23 | 8.60 |
| Tensile strength/Mpa | 24.5 | 22.1 | 19.1 | 15.6 | 11.0 | 8.6 |
| Elongation at break/% | 1250 | 1030 | 800 | 690 | 500 | 450 |
| Tear strength/N/m | 115 | 112 | 81 | 58 | 32 | 25 |
Embodiment 2: with junked tire and the broken waste rubber powder that gets of scrap rubber shoe powder, cross 5 mesh sieves, waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron, with the microwave desulfurization jar of packing into of the waste rubber powder behind de-iron bits and the impurity, add Rubber Softener turps, press mass ratio, waste rubber powder: Rubber Softener turps=100: 5; The microwave heating desulfurization, 220 ℃ of Heating temperatures; After desulfurization is finished, be cooled to below 150 ℃ roller refining, slice.The kind of waste old comprises natural rubber, styrene-butadiene rubber(SBR), cis-1,4-polybutadiene rubber etc.The microwave frequency of the microwave that is adopted is 1000MHz, and microwave intensity is 0.25KWh/Kg, and the microwave desulfurization time is 20min.
Embodiment 3: with the scrap stock that produce in junked tire, scrap rubber footwear and the rubber tyre production process and waste material pulverize waste rubber powder, cross 80 mesh sieves, waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron, with the microwave desulfurization jar of packing into of the waste rubber powder behind de-iron bits and the impurity, add the Rubber Softener Yatall MA, press mass ratio, waste rubber powder: Rubber Softener Yatall MA=100: 1; The microwave heating desulfurization, 170 ℃ of Heating temperatures; After desulfurization is finished, be cooled to below 150 ℃ roller refining, slice.The kind of waste old comprises natural rubber, cis-1,4-polybutadiene rubber, chloroprene rubber and paracril etc.The microwave frequency of the microwave that is adopted is 945MHz, and microwave intensity is 0.1KWh/Kg, and the microwave desulfurization time is 25min.
Embodiment 4: with the scrap stock that produce in junked tire, waste tape and the rubber boots production process and waste material pulverize waste rubber powder, cross 100 mesh sieves, waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron, with the microwave desulfurization jar of packing into of the waste rubber powder behind de-iron bits and the impurity, add Rubber Softener rosin and di-terpene, press mass ratio, waste rubber powder: Rubber Softener rosin and di-terpene=100: 10; The microwave heating desulfurization, 140 ℃ of Heating temperatures; After desulfurization is finished, be cooled to below 140 ℃ roller refining, slice leaving standstill cooling under the condition of secluding air.The kind of waste old comprises natural rubber, styrene-butadiene rubber(SBR), isoprene-isobutylene rubber and paracril etc.The microwave frequency of the microwave that is adopted is 915MHz, and microwave intensity is 1.0KWh/Kg, and the microwave desulfurization time is 40min.
Embodiment 5: with the scrap stock that produce in junked tire, scrap rubber footwear and the rubber tyre production process and waste material pulverize waste rubber powder, cross 200 mesh sieves, waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron, with the microwave desulfurization jar of packing into of the waste rubber powder behind de-iron bits and the impurity, add Rubber Softener coal tar and heavy oil, press mass ratio, waste rubber powder: Rubber Softener coal tar and heavy oil=100: 8; The microwave heating desulfurization, 300 ℃ of Heating temperatures; After desulfurization was finished, water spray was cooled to below 150 ℃, roller refining, slice.The kind of waste old comprises natural rubber, isoprene-isobutylene rubber and paracril etc.The microwave frequency of the microwave that is adopted is 1500MHz, and microwave intensity is 0.5KWh/kg, and the microwave desulfurization time is 30min.
Embodiment 6: with the scrap stock that produce in junked tire, scrap rubber footwear and the rubber tyre production process and waste material pulverize waste rubber powder, cross 150 mesh sieves, waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron, with the microwave desulfurization jar of packing into of the waste rubber powder behind de-iron bits and the impurity, the microwave heating desulfurization, 250 ℃ of Heating temperatures; After desulfurization is finished, be cooled to below 150 ℃ roller refining, slice.The kind of waste old comprises isoprene-isobutylene rubber and paracril etc.The microwave frequency of the microwave that is adopted is 2450MHz, and microwave intensity is 0.65KWh/Kg, and the microwave desulfurization time is 35min.
Embodiment 7: with the scrap stock that produce in junked tire, scrap rubber footwear and the rubber tyre production process and waste material pulverize waste rubber powder, cross 100 mesh sieves, waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron, with the microwave desulfurization jar of packing into of the waste rubber powder behind de-iron bits and the impurity, add Rubber Softener Stockholm tar and heavy oil, press mass ratio, waste rubber powder: Rubber Softener Stockholm tar and heavy oil=100: 6; The microwave heating desulfurization, 200 ℃ of Heating temperatures; After desulfurization was finished, water spray was cooled to below 150 ℃, roller refining, slice.The kind of waste old comprises natural rubber, cis-1,4-polybutadiene rubber and paracril etc.The microwave frequency of the microwave that is adopted is 945MHz, and microwave intensity is 0.45KWh/kg, and the microwave desulfurization time is 28min.
Claims (10)
1. adopt the reclaimed rubber preparation method of microwave desulfurization, it is characterized in that it may further comprise the steps:
1) the waste old material is pulverized waste rubber powder, cross 5～200 mesh sieves;
2) waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron;
3) waste rubber powder behind de-iron bits and the impurity is packed into microwave desulfurization jar, the adding Rubber Softener is pressed mass ratio, waste rubber powder: Rubber Softener=100: 0～15;
4) microwave heating desulfurization, 140～300 ℃ of Heating temperatures;
5) after desulfurization is finished, be cooled to below 150 ℃ roller refining, slice.
2. the reclaimed rubber preparation method of employing microwave desulfurization as claimed in claim 1 is characterized in that the waste old material package draws together damaged tire, scrap rubber footwear and waste tape rubber item, and scrap stock that produce in the rubber production process and waste product.
3. the reclaimed rubber preparation method of employing microwave desulfurization as claimed in claim 1 or 2 is characterized in that the kind of waste old comprises natural rubber, styrene-butadiene rubber(SBR), cis-1,4-polybutadiene rubber, isoprene-isobutylene rubber, chloroprene rubber and paracril.
4. the reclaimed rubber preparation method of employing microwave desulfurization as claimed in claim 1, the microwave frequency that it is characterized in that described microwave is 915～2450MHz.
5. the reclaimed rubber preparation method of employing microwave desulfurization as claimed in claim 4, the microwave frequency that it is characterized in that described microwave is 945MHz.
6. as the reclaimed rubber preparation method of claim 1 or 4 or 5 described employing microwave desulfurizations, it is characterized in that described microwave intensity is 0.1～1.0KWh/Kg.
7. as the reclaimed rubber preparation method of claim 1 or 4 or 5 described employing microwave desulfurizations, it is characterized in that the described microwave desulfurization time is 5～40min.
8. the reclaimed rubber preparation method of employing microwave desulfurization as claimed in claim 1 is characterized in that described Heating temperature is 160～180 ℃.
9. the reclaimed rubber preparation method of employing microwave desulfurization as claimed in claim 1 is characterized in that described Rubber Softener is selected from least a in Stockholm tar, Yatall MA, turps, rosin, di-terpene, coal tar, the heavy oil.
10. the reclaimed rubber preparation method of employing microwave desulfurization as claimed in claim 1, it is characterized in that described cooling be selected under the condition of secluding air, leave standstill the cooling or spray cooling.
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| CN101235161B (en) * | 2008-02-26 | 2010-07-14 | 刘昌志 | Rubber microwave regeneration linkage device |
| CN101824173A (en) * | 2010-03-23 | 2010-09-08 | 江汉大学 | Microwave modified rubber powder of waste tire and preparation method thereof |
| CN101633746B (en) * | 2009-08-27 | 2011-05-11 | 福建环科化工橡胶集团有限公司 | Method for preparing environment-friendly fine butyl renewable rubber |
| CN102127246A (en) * | 2010-12-13 | 2011-07-20 | 四川大学 | Method for removing miscellaneous elements from waste high polymer material by using microwave irradiation |
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| CN102219923A (en) * | 2011-04-15 | 2011-10-19 | 金秋南 | Process for preparing reduced rubber by utilizing environmentally-friendly waste tyre |
| CN102295791A (en) * | 2011-05-23 | 2011-12-28 | 浙江力源化工有限公司 | High-strength reclaimed rubber |
| CN102753328A (en) * | 2010-01-31 | 2012-10-24 | 恩特克斯拉斯特及米施克有限责任公司 | Devulcanization of scrap rubber |
| CN103059889A (en) * | 2013-01-23 | 2013-04-24 | 中国矿业大学 | Microwave pretreatment desulfurization coking method and device |
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| CN101235161B (en) * | 2008-02-26 | 2010-07-14 | 刘昌志 | Rubber microwave regeneration linkage device |
| CN101633746B (en) * | 2009-08-27 | 2011-05-11 | 福建环科化工橡胶集团有限公司 | Method for preparing environment-friendly fine butyl renewable rubber |
| CN102753328B (en) * | 2010-01-31 | 2015-02-25 | 恩特克斯拉斯特及米施克有限责任公司 | Devulcanization of scrap rubber |
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| WO2011096004A1 (en) * | 2010-02-05 | 2011-08-11 | O.R.P. S.R.L. | Process for the manufacture of bituminous conglomerates |
| CN101824173B (en) * | 2010-03-23 | 2012-09-05 | 江汉大学 | Microwave modified rubber powder of waste tire and preparation method thereof |
| CN101824173A (en) * | 2010-03-23 | 2010-09-08 | 江汉大学 | Microwave modified rubber powder of waste tire and preparation method thereof |
| CN102127246A (en) * | 2010-12-13 | 2011-07-20 | 四川大学 | Method for removing miscellaneous elements from waste high polymer material by using microwave irradiation |
| CN102127246B (en) * | 2010-12-13 | 2013-02-06 | 四川大学 | Method for removing miscellaneous elements from waste high polymer material by using microwave irradiation |
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| CN102219923A (en) * | 2011-04-15 | 2011-10-19 | 金秋南 | Process for preparing reduced rubber by utilizing environmentally-friendly waste tyre |
| CN102295791A (en) * | 2011-05-23 | 2011-12-28 | 浙江力源化工有限公司 | High-strength reclaimed rubber |
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